CN220194829U - Narrow-distribution heterogeneous reaction device - Google Patents
Narrow-distribution heterogeneous reaction device Download PDFInfo
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- CN220194829U CN220194829U CN202321903834.4U CN202321903834U CN220194829U CN 220194829 U CN220194829 U CN 220194829U CN 202321903834 U CN202321903834 U CN 202321903834U CN 220194829 U CN220194829 U CN 220194829U
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- separator
- component separator
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 46
- 238000009826 distribution Methods 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 3
- 239000011552 falling film Substances 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 238000000199 molecular distillation Methods 0.000 claims description 3
- 238000007790 scraping Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 238000005728 strengthening Methods 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 239000004094 surface-active agent Substances 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 4
- 239000012847 fine chemical Substances 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 description 15
- 239000003999 initiator Substances 0.000 description 13
- 239000000047 product Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000376 reactant Substances 0.000 description 5
- 238000000746 purification Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 241000353097 Molva molva Species 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004807 desolvation Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 ethoxyl Chemical group 0.000 description 1
- 239000003828 free initiator Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to the field of fine chemical equipment, in particular to a narrow-distribution heterogeneous reaction device which comprises a main reactor, a primary component separator, a secondary component separator, a heat exchanger, a complete condenser, a primary light component collector, a secondary heavy component collector, a secondary light component collector, a material pump and a circulating pump, wherein the main reactor is a closed-loop reactor; the narrow-distribution heterogeneous reaction device greatly improves the purity and molecular weight distribution trend of the surfactant product of gas-liquid-solid heterogeneous synthesis and improves the quality of the product.
Description
Technical Field
The utility model relates to the field of fine chemical equipment, in particular to a narrow-distribution heterogeneous reaction device.
Background
In the technical field of fine chemical engineering, the existing synthesis preparation surfactants, in particular to a gas-solid-liquid-solid heterogeneous reaction device for anionic surfactants and nonionic surfactants, which mostly adopts an external circulation or kettle type stirring mode to finish the phase reaction synthesis process, and few surfactant products prepared by adopting continuous pipelines gradually reduce the conversion rate along with the increase of relative molecular mass.
When solvents, moisture, cocatalysts are introduced during the synthesis process, or the polymerization degree range is broadened due to controlled conditions, the purity and molecular weight distribution of the surfactant product are further affected.
Chinese utility model patent: CN207169663U, an external circulation ethoxyl addition reaction device, although the circulation type gas-liquid spraying reaction can strengthen the gas-liquid two-phase mass transfer efficiency, the solvent, moisture or oligomer in the reaction process cannot be effectively separated, and the obtained product distribution is still wider.
Disclosure of Invention
The utility model aims to solve the technical defects and provides a narrow-distribution heterogeneous reaction device which can purify materials in the reaction process so as to improve the purity of heterogeneous synthetic reactants and improve the distribution of the molecular weight of products.
The utility model discloses a narrow-distribution heterogeneous reaction device, which comprises a main reactor, a primary component separator, a secondary component separator, a heat exchanger, a total condenser, a primary light component collector, a secondary heavy component collector, a secondary light component collector, a material pump and a circulating pump, wherein the primary component separator is arranged on the main reactor; the bottom of the primary reactor is connected with the inlet of the material pump; the outlet of the material pump is respectively connected with the primary component separator, the secondary component separator and the top feed inlet of the main reactor; the bottom of the main reactor is connected with the inlet of the circulating pump; the circulating pump outlet is respectively connected with the heat exchanger, the primary component separator and the feed inlet of the secondary component separator; the top outlet of the heat exchanger is connected with the top material inlet of the main reactor; the side part of the primary component separator is provided with a full condenser, the bottom of the full condenser is connected with a primary light component collector, and the bottom of the primary component separator is respectively connected with inlets of the primary reactor, the main reactor and the secondary component separator; the bottom of the first-stage light component collector is connected with the primary reactor; the bottom of the secondary component separator is respectively connected with the tops of the secondary heavy component collector and the secondary light component collector; the bottoms of the secondary heavy component collector and the secondary light component collector are connected with the inlet of the main reactor.
The primary reactor, the material pump and the primary component separator form a pretreatment circulation loop.
The main reactor, the circulating pump, the heat exchanger, the primary component separator and the secondary component separator form a reaction and post-treatment circulating loop.
The primary reactor is a kettle type reactor or a fluidized bed reactor with stirring function, and the stirring mode is mechanical stirring or magnetic stirring. When the operating pressure is more than 0 and less than 0.1MPa, the treatment temperature is more than or equal to 0 and less than or equal to 150 ℃, and the material to be treated is non-dangerous chemical, mechanical stirring is preferred. When the operating pressure P is more than or equal to 0.1MPa and the material to be treated belongs to dangerous chemicals or the treatment process relates to dangerous chemical technology, magnetic stirring is preferred. The primary reactor can realize solid raw material conversion, catalytic activation of reaction materials, preparation of reaction intermediates, preparation of high-viscosity high-molecular polymers and the like, and is a commercial product in the prior art, and specific structures are not repeated here.
The main reactor is a kettle reactor with an external circulation system and a built-in jet mass transfer strengthening member. The external circulation can be used for preparing a single circulation loop or a double circulation loop according to the growth ratio of the synthetic substrate and the quality grade of the product, and is mainly used for realizing gas-liquid heterogeneous reaction. The main reactor, the circulating pump and the heat exchanger are all commercial products in the prior art, and specific structures are not repeated here.
The primary component separator is a thin film distillation device, the operating temperature of which is more than 0 and less than or equal to 150 ℃, and is mainly used for separating and recovering water and volatile solvents or other auxiliary agents in the whole heterogeneous reaction process.
The secondary component separator is a molecular distillation device with a scraping plate or falling film structure, the operation temperature is 150 < T < 300 ℃, preferably 150 < T < 250 ℃, and the secondary component separator is mainly used for separating free initiator and low molecular weight polymer of heterogeneous reaction products.
The first-stage light component collector, the second-stage heavy component collector and the second-stage light component collector are stainless steel storage tanks for collecting solvents and low-molecular-weight polymers with different volatilities and different free ranges.
The narrow-distribution heterogeneous reaction device greatly improves the purity and molecular weight distribution trend of the surfactant product of gas-liquid-solid heterogeneous synthesis and improves the quality of the product.
Compared with the prior art, the utility model can obtain the following technical effects:
1. the heterogeneous reaction which is carried out by the high solidifying point initiator is needed, after the material melting treatment, the catalytic activation or the solvent dissolution treatment and the like are carried out by the primary reactor, the heterogeneous reaction efficiency can be improved, the activated initiator can remove the solvent, the moisture and the like by a primary component separator, the reactive substrate can be purified, and the collected solvent can be recycled.
2. For the initiator which is easy to sublimate when being heated, such as phenols, a solvent is needed to be added to inhibit the sublimation of the initiator when being heated, and redundant solvent can be processed in cascade through a primary component separator and a secondary component separator in the later period of heterogeneous reaction to be separated and recovered, so that the phenomenon of reduced reaction efficiency caused by sublimation and crystallization of the initiator is effectively prevented.
3. The whole process is closed, the volatility of the separated components is matched with the average free path according to the gradient of the operation temperature, the whole safety of the device and the repeated utilization rate of process auxiliary agents are improved, and the whole environmental protection and the operation cost are reduced.
4. Compact equipment layout, and the intensive and modularized control management of heterogeneous reaction and post-treatment is realized.
5. The first-stage component separator and the second-stage component separator are arranged in a cascade manner, so that the influence of water, solvent and auxiliary agent in the early stage of the reaction on the molecular weight distribution in the heterogeneous reaction process is effectively reduced, and the purification of reactants and the narrowing of the molecular weight distribution are further realized through the separation of the low-molecular-weight polymer in the later stage.
6. The process is easy to realize automatic control, the production amount of VOCs is extremely low, the color and luster of the product are good, the quality is excellent, and the method is more suitable for the application in the industries and fields of medicines, chemical intermediates, cosmetics, new energy sources, electronics and the like.
Drawings
Fig. 1 is a schematic structural view of the present utility model.
Detailed Description
In order to further describe the technical means and effects adopted by the present utility model for achieving the intended purpose, the following detailed description will refer to the specific implementation, structure, characteristics and effects according to the present utility model with reference to the accompanying drawings and preferred embodiments.
Example 1:
as shown in fig. 1, the utility model discloses a narrow-distribution heterogeneous reaction device, which comprises a main reactor 2, a primary reactor 1, a primary component separator 6, a secondary component separator 7, a heat exchanger 3, a total condenser 11, a primary light component collector 8, a secondary heavy component collector 9, a secondary light component collector 10, a material pump 5 and a circulating pump 4; the bottom of the primary reactor 1 is connected with the inlet of a material pump 5; the outlet of the material pump 5 is respectively connected with the primary component separator 6, the secondary grouping separator 7 and the top feed inlet of the main reactor 2; the bottom of the main reactor 2 is connected with the inlet of the circulating pump 4; the outlet of the circulating pump 4 is respectively connected with the feed inlets of the heat exchanger 3, the primary component separator 6 and the secondary component separator 7; the top outlet of the heat exchanger 3 is connected with the top material inlet of the main reactor 2; the side part of the primary component separator 6 is provided with a full condenser 11, the bottom of the full condenser 11 is connected with the primary light component collector 8, and the bottom of the primary component separator 6 is respectively connected with the inlets of the primary reactor 1, the main reactor 2 and the secondary grouping separator 7; the bottom of the first-stage light component collector 8 is connected with the primary reactor 1; the bottom of the secondary grouping separator 7 is respectively connected with the tops of the secondary heavy component collector 9 and the secondary light component collector 10; the bottoms of the secondary heavy component collector 9 and the secondary light component collector 10 are connected with the inlet of the main reactor 2.
The primary reactor 1, the material pump 5 and the primary component separator 6 form a pretreatment circulation loop.
The main reactor 2, the circulating pump 4, the heat exchanger 3, the primary component separator 6 and the secondary grouping separator 7 form a reaction and post-treatment circulating loop.
The primary reactor 1 is a kettle type reactor or a fluidized bed reactor with stirring function, and the stirring mode is magnetic stirring.
The main reactor 2 is a kettle reactor with an external circulation system and a built-in jet mass transfer strengthening member.
The primary component separator 6 is a thin film distillation apparatus.
The secondary grouping separator 7 is a molecular distillation device with a scraping plate or falling film structure.
The primary light component collector 8, the secondary heavy component collector 9 and the secondary light component collector 10 are stainless steel storage tanks.
The circulating pump 4 and the material pump 5 are high-viscosity materials and are centrifugal pumps provided with sealed monitoring siphon tanks, the heat exchanger 3 is a tube type heat exchanger 3, the primary component separator 6 and the secondary component separator 7 are heated by heat conduction oil, the low temperature Leng Jingche is hot, a Roots vacuum unit is arranged, and the operating pressure is 5-30 PaG.
Control valves on connecting pipelines between the components in fig. 1 are not shown, and are arranged in a practical device according to requirements so as to realize one-way on-demand operation of materials.
The following are three different reaction processes in the production process of the device of this example:
reaction 1:
the solid phase initiator (alcohol, phenol, ether, acid, ester and amine) is mixed with solvent, catalyst and promoter in the primary reactor 1, and is heated and dissolved under the protection of nitrogen, the operation temperature is 60-150 ℃ and the operation pressure is-0.02-0.15 MPa. The activated initiator is sent to a primary component separator 6 to remove water and solvent by a material pump 5, and the operation temperature is 80-120 ℃. The solvent-removed initiator enters a main reactor 2 to react with gaseous or liquid reactants at the reaction temperature of 120-200 ℃ and the reaction pressure of-0.02-1.0 MPa. Curing for 1-2 h after the reaction is finished, and delivering the reaction solution to a secondary component separator 7 through a circulating pump 4 to remove low molecular weight polymer, wherein the operation temperature is 150-300 ℃. And after purification, cooling to 60-80 ℃ and discharging.
Reaction 2:
the solid phase initiator (alcohol, phenol, ether, acid, ester and amine) is mixed with solvent, catalyst and promoter in the primary reactor 1, and is heated and dissolved under the protection of nitrogen, the operation temperature is 60-150 ℃ and the operation pressure is-0.02-0.15 MPa. The activated initiator is sent to the main reactor 2 through a material pump 5 to react with gaseous or liquid reactants at the temperature of 120-200 ℃ and the reaction pressure of-0.02-1.0 MPa. Curing for 1-2 h after the reaction is finished, and delivering the reaction liquid to a primary component separator 6 through a circulating pump 4 to remove light components, wherein the operation temperature is 60-150 ℃. Then enters a secondary component separator 7 to remove low molecular weight polymer, and the operation temperature is 150-300 ℃. And after purification, cooling to 60-80 ℃ and discharging.
Reaction 3:
the solid phase initiator (alcohol, phenol, ether, acid, ester and amine) is mixed with solvent, catalyst and promoter in the primary reactor 1, and is heated and dissolved under the protection of nitrogen, the operation temperature is 60-150 ℃ and the operation pressure is-0.02-0.15 MPa. The activated initiator is sent to a primary component separator 6 to remove water and solvent by a material pump 5, and the operation temperature is 80-120 ℃. The activated initiator after desolvation returns to the primary reactor 1 again to react with gaseous or liquid reactants at the temperature of 120-200 ℃ and the reaction pressure of-0.02-1.0 MPa. Curing for 1-2 h after the reaction is finished, and delivering the reaction liquid to a secondary component separator 7 through a material pump 5 to remove low molecular weight polymer, wherein the operation temperature is 150-300 ℃. And after purification, cooling to 60-80 ℃ and discharging.
In the description of the present application, it should be understood that the terms "center," "longitudinal," "transverse," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," etc. indicate or are based on the orientation or positional relationship shown in the drawings, merely for convenience of description and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present application. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the description of the present application, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; may be a mechanical connection; can be directly connected or indirectly connected through an intermediate medium, and can be in interaction relationship with two elements. The specific meaning of the terms in this application will be understood by those of ordinary skill in the art as the case may be.
In this application, unless expressly stated or limited otherwise, a first feature "above" or "below" a second feature may include both the first and second features being in direct contact, and may also include the first and second features not being in direct contact but being in contact with each other by way of additional features therebetween. Moreover, a first feature being "above," "over" and "on" a second feature includes the first feature being directly above and obliquely above the second feature, or simply indicating that the first feature is higher in level than the second feature. The first feature being "under", "below" and "beneath" the second feature includes the first feature being directly under and obliquely below the second feature, or simply means that the first feature is less level than the second feature.
The present utility model is not limited to the preferred embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present utility model.
Claims (6)
1. A narrow-distribution heterogeneous reaction device comprises a main reactor and is characterized in that: the system also comprises a primary reactor, a primary component separator, a secondary component separator, a heat exchanger, a complete condenser, a primary light component collector, a secondary heavy component collector, a secondary light component collector, a material pump and a circulating pump; the bottom of the primary reactor is connected with the inlet of the material pump; the outlet of the material pump is respectively connected with the primary component separator, the secondary component separator and the top feed inlet of the main reactor; the bottom of the main reactor is connected with the inlet of the circulating pump; the circulating pump outlet is respectively connected with the heat exchanger, the primary component separator and the feed inlet of the secondary component separator; the top outlet of the heat exchanger is connected with the top material inlet of the main reactor; the side part of the primary component separator is provided with a full condenser, the bottom of the full condenser is connected with a primary light component collector, and the bottom of the primary component separator is respectively connected with inlets of the primary reactor, the main reactor and the secondary component separator; the bottom of the first-stage light component collector is connected with the primary reactor; the bottom of the secondary component separator is respectively connected with the tops of the secondary heavy component collector and the secondary light component collector; the bottoms of the secondary heavy component collector and the secondary light component collector are connected with the inlet of the main reactor.
2. A narrow distribution heterogeneous reaction device according to claim 1, characterized in that: the primary reactor is a kettle type reactor or a fluidized bed reactor with stirring function, and the stirring mode is mechanical stirring or magnetic stirring.
3. A narrow distribution heterogeneous reaction device according to claim 1, characterized in that: the main reactor is a kettle reactor with an external circulation system and a built-in jet mass transfer strengthening member.
4. A narrow distribution heterogeneous reaction device according to claim 1, characterized in that: the primary component separator is a thin film distillation device.
5. A narrow distribution heterogeneous reaction device according to claim 1, characterized in that: the secondary component separator is a molecular distillation device with a scraping plate or falling film structure.
6. A narrow distribution heterogeneous reaction device according to claim 1, characterized in that: the first-stage light component collector, the second-stage heavy component collector and the second-stage light component collector are stainless steel storage tanks.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321903834.4U CN220194829U (en) | 2023-07-19 | 2023-07-19 | Narrow-distribution heterogeneous reaction device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321903834.4U CN220194829U (en) | 2023-07-19 | 2023-07-19 | Narrow-distribution heterogeneous reaction device |
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| Publication Number | Publication Date |
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| CN220194829U true CN220194829U (en) | 2023-12-19 |
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| CN202321903834.4U Active CN220194829U (en) | 2023-07-19 | 2023-07-19 | Narrow-distribution heterogeneous reaction device |
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